関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Pyrazinecarboxylic acid | HCID 1047 | — |
| 反応物 | N-Hydroxysuccinimide | HCID 80170 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[3-(2-Pyrazinecarbonylamino)propylthio]pyridine | HCID 15231502 | 34% |
反応手順
To a solution of 1.00 g (8.06 mmol) of 2-pyrazinecarboxylic acid and 1.21 g (10.5 mmol) of N-hydroxysuccinimide in 70 ml of methylene-chloride, 1.85 g (9.67 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (WSC) was added with stirring under ice-cooling, and the mixture was stirred at room temperature for 1 hour. Further, 1.94 g (8.06 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride was added, and the mixture was stirred at room temperature for 3 hours. The reaction mixture was washed with saturated aqueous sodium bicarbonate and water, and dried. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate) to give 0.751 g of the desired compound (34.0% yield, colorless powder).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05246948 |
|---|
| 出典データセット | uspto-grants-1993_09 |
|---|
| ORD ID | ord-d55965f78437450f9aef72b94ae9f168 |
|---|
| 出典メモ | uspto-grants-1993_09 |
|---|